高分辨电感耦合等离子体磁质谱法测定含铜不锈钢中痕量磷

作者通过试验,用电感耦合等离子体磁质谱(HR-ICP-MS)测定含铜不锈钢中磷含量时,采用高分辨率模式,选择分辨率为4000,在此条件下磷峰可与干扰双原子分子或离子的峰分开。又通过以含铁基的磷标准溶液优化了气体流量和离子透镜的参数,使磷的信号值提高至3×105cps。而加入45Sc作为内标元素又可显著提高测定的稳定性。分别用不锈钢样品和纯铁粉作基体,加入标准溶液制作标准曲线。结果表明:两种方法的线性均较好,分别测得实际样品的结果及其相对标准偏差也基本一致。但两种方法的检出限(3s)不同,前者为1.0μg·g^-1,后者为0.18μg·g^-1。所提出方法的样品处理过程如下:称取样品0.10g置于消解罐中,加入盐酸溶液2mL及硝酸溶液1mL,待剧烈反应缓解时,将消解罐加盖并置于微波消解仪中,于100℃消解10min,升温至200℃继续消解20min。冷却后将溶液转移至100 mL石英容量瓶中,加入0.2mg·L^-1钪内标溶液1mL,加水至刻度,摇匀。此溶液在仪器工作条件下进行HR-ICP-MS测定。对含磷51μg·g^-1的含铜不锈钢,按本方法测定所得结果的相对标准偏差(n=10)小于4%。应用本方法分析了7种标准物质或已知样品(包括低合金钢、含铜不锈钢、高温合金),并同时用ICP-AES进行校对分析。结果表明,本方法与ICP-AES的测定结果基本一致。但本方法的结果与标准物质的认定值更接近,而且对低含量磷(9μg·g^-1)也可很好测定。     

Advances in theoretical study on transition-metal-catalyzed C−H activation

Transition-metal-catalyzed C–H activation represents one of most attractive research fields in modern organic chemistry while theoretical studies have become a popular and effective tool for elucidating mechanism nowadays. The recent achievements in the cross field of the two orientations are reviewed in this article. The first part introduced the advances in theoretical study on transition-metal-catalyzed C–H activation. The elegant work reported mainly in and after 2013, classified according to the mechanisms of C–H activation, were covered. The second part provided an analysis on the distribution of quantum-chemical methods, solvation models and basis sets in the collected theoretical studies.     

PEO/PVDF-based gel polymer electrolyte by incorporating nano-TiO2 for electrochromic glass

Journal of Sol-Gel Science and Technology - To develop high performance mixed matrix gel polymer electrolyte, the synergistic effect of blending PVDF (PEO/PVDF weigh ratio of 85:15) and adding...     

Fabrication and electrochemistry study of multi-thiol coronary molecule monolayers

Single-component monolayer of novel multi-thiol coronary molecule and two-component mixed monolayer composed of coronary molecule and n-alkanethiol on gold substrates are described. The assembly of monolayers is characterized by ellipsometry, infrared spectroscopy and X-ray photoelectron spectroscope. The electrochemical properties of the single- and two-component monolayers are evaluated by cyclic voltammetry and electrochemical impedance spectroscopy experiments. Coronary molecule with multi-thiol groups has the ability to form stable monolayer via the interaction of mercapto groups and Au surface. Electrochemical impedance measurements indicate that 89.9% of the gold surface is blocked by the coronary molecule, which is attributed to the special spatial structure of the coronary molecule. The uncovered site on gold surface in coronary molecule monolayer could be occupied by the second suitable molecule. The mixed monolayer prepared by stepwise assembly of coronary molecule and n-alkanethiol has complete compact packing and few defects.     

现代地貌过程中的人类作用

人为的风化、侵蚀、搬运、堆积、造貌等作用，是现代地貌过程中一种新的营力。这种作用的强度主要取决于人口、社会经济发展水平、科学技术水平等因素。而人为地貌作用导致的地貌环境变化又会对人类社会发展产生正负两方面的影响，尤其是其负面影响常常会产生与人们的主观愿望相反的效果。因此，必须根据可持续发展战略来处理人类与地貌环境的关系。     

Nd（i－PrO）_2Cl－AlEt_3均相二元催化剂异戊二烯聚合动力学──Ⅲ．AlEt_3的链转移作用

Ｎｄ（ｉ－ＰｒＯ）_２Ｃｌ－ＡｌＥｔ_３均相二元催化剂异戊二烯聚合动力学──Ⅲ．ＡｌＥｔ_３的链转移作用蔡小平，龚志，王佛松朱行洁，李秀华（中国科学院长春应用化学研究所长春１３００２２）（吉林化工集团公司研究院吉林）关键词异戊二烯，聚合动力学，均相催化...     

非线性激光场中量子噪声之间的耦合效应

用二维气体激光模型对量子噪声的实部和虚部存在耦合的激光场进行了理论分析，通过福克－普朗克方程导出了定态激光光场强度和位相的分布函数，算出了定态激光强度和位相的平均值，方差和偏斜度，与量子噪声的两个分量为独立随机变量的激光场相比，噪声间的耦合极大地改变了激光场强度和位相的涨落，并引起了激光场强度与位相之间的耦合。     

Preparation of GaN-based cross-sectional TEM specimens by laser lift-off

Laser lift-off (LLO) technology is successfully used to prepare GaN-based TEM cross-sectional specimens. Detailed procedures of the method to prepare the specimens are demonstrated. Large thin areas suitable for TEM analysis were obtained. TEM images of the resulting GaN interface are studied, and the changes in structural quality are confined to approximately the first 250 nm of the epilayer. Clear TEM images of the whole epilayer and the InGaN quantum wells and the HRTEM images of the superlattice layer are demonstrated, showing that LLO is a quick and ideal method to study the crystal structure of the epilayer, especially if only the upper layers are of interest.     

Strong electronic coupling between dimolybdenum units linked by the N,N'-dimethyloxamidate anion in a molecule having a heteronaphthalene-like structure

Very strong electronic communication, manifested in a K(C) value of ca. 10(9), has been found in a system of three compounds separated by one electron oxidation where each compound contains two metal-metal bonded Mo(2)(n+) units linked by a dimethyloxamidate anion, CH(3)N(O)C-C(O)NCH(3)(2)(-). The Mo-Mo distances increase as the oxidation state increases and the bond order decreases, while the diamagnetic, doubly oxidized species becomes essentially planar and resembles a naphthalene molecule. Calculations at the DFT level indicate that a strong transition in the near-IR region, shown by the singly oxidized and paramagnetic species, is best described as a HOMO-1 --> SOMO transition.     

Synthesis and structure of Zn7(mu4-O)2(OAc)10(Pz)2(OAc = acetate; Pz = pyrazine)

Reaction of Zn(OAc)(2).2H(2)O with pyrazine in refluxing ethanol gives the unusual heptanuclear complex Zn7(mu4-O)(2)(OAc)(10)(Pz)(2) (1) (OAc = acetate, Pz = pyrazine) in 46% yield. A single-crystal X-ray diffraction study of revealed a central Zn(7) core in which two pseudo-tetrahedral Zn(4) units are joined at a common vertex. The two pyrazine molecules are bound as terminal (eta1) ligands.